Electrochemistry

Operando multi-modal imaging with bulk-level electrochemical data

Electrochemical characterization tool selector

Nano-Manipulator Biasing TEM Tomography TEM Liquid TEM Gas TEM Liquid X-Ray Liquid SEM
Battery Configuration Individual nanowire/nanoparticle
Thin film
Imaging Higher resolution and diffraction
EDS/EELS compatibility
3D reconstruction
In-situ imaging
Pre-and post-mortem analysis
Transfer air-sensitive samples
Thermal cycling
Beam Effects Compatibility with volatile electrolytes
Minimal beam damage
Quantitative Electrochemistry Replicate bulk measurements
Image all battery components
Longer cycling

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Bulk Electrochemistry in TEM

Replicating bulk electrochemistry data in TEM

Hummingbird Scientific’s newest Generation V in-situ liquid-electrochemistry TEM holder allows researchers for the first time to fully replicate bulk-level electrochemical details inside the transmission electron microscope. A newly developed hardware and cells allows quantitative measurements of electrochemical processes with details showing the complete electrochemical cycle, replicating the data of bulk samples.

As illustrated, a cyclic voltammetry (CV) study of a model compound 01.M copper sulfate showing plating and deposition of copper has been presented here. The copper deposition and stripping occurs at the Pt working electrode, mimicking bulk behavior.

 

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* Grujicic, D. and Pesic, B; Electrochimica Acta 47 (2002) 2901-2912. Image copyright © 2002 Elsevier Science Ltd.

Electrochemistry Video Spotlight

Origin of Li charging and discharging of primary particles

Using Hummingbird Scientific liquid cell technology, Dr. William Chueh and his team at Stanford University built a transparent nano-battery in the synchrotron liquid-electrochemistry x-ray platform, taking advantage of the modularity of the tip design.

The video shows the evolution of Li composition for particles during lithiation at a rate of 2C. The hue represents the Li composition X, where red indicate X=1 and green indicate X=0. The brightness represents thickness of material. The position of each particle (outlined in white) relative to each other, and the dashed line indicates divisions. These results highlight the crucial role of surface reaction rate for lithiation, observing these inconsistencies of ion insertion have implications for electrode engineering and battery management for future generation battery technology.

Reference: J. Lim,Y. Li, D. H. Alsem, H. So, S. C. Lee, P. Bai, D.A. Cogswell, X. Liu, N. Jin, Y. Yu, N. J. Salmon, D. A. Shapiro, M. Z. Bazant, T.Tyliszczak, W. C. Chueh, “Origin and Hysteresis of Lithium Compositional Spatiodynamics Within Battery Primary Particles,” Science 353 (2016) pp. 566-571 Abstract

Movie copyright © 2016, American Association for the Advancement of Science

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Selected Electrochemistry Publications

Nikhilendra Singh, Timothy S. Arthur, Oscar Tutusaus, Jing Li, Kim Kisslinger, Huolin L. Xin, Eric A. Stach, Xudong Fan, and Rana Mohtadi. “Achieving High Cycling Rates via In-situ Generation of Active Nanocomposite Metal Anodes.” ACS Applied Energy Materials (2018) Abstract
Mei Sun, Xing Li, Zhiqiang Tang, Xianlong Wei and Qing Chen. “Constant-Rate Dissolution of InAs Nanowires in Radiolytic Water Observed by In situ Liquid Cell TEM.” Nanoscale (2018) Abstract
Khim Karki, Tyler Mefford, Daan Hein Alsem, Norman Salmon and William C. Chueh. “Replicating Bulk Electrochemistry in Liquid Cell Microscopy.” Microscopy & Microanalysis (2018) Abstract
Jeung Hun Park, Tommy Watanabe, Ainsley Pinkowitz, David J. Duquette, Robert Hull, Daniel A. Steingart and Frances M. Ross. “In situ EC-TEM Studies of Metal Thin Film Corrosion in Liquid Solutions at Elevated Temperatures.” Microscopy & Microanalysis (2018) Abstract
Chen Houa, Jiuhui Hanb, Pan Liua, Chuchu Yangb, Gang Huangb, Takeshi Fujitab, Akihiko Hiratab, and Mingwei Chen. “Operando observations of RuO2 catalyzed Li2O2 formation and decomposition in a Li-O2 micro-battery,” Nano Energy (2018) Abstract
Pan Liu, Jiuhui Han, Xianwei Guo, Yoshikazu Ito, Chuchu Yang, Shoucong Ning, Takeshi Fujita, Akihiko Hirata and Mingwei Chen. “Operando characterization of cathodic reactions in a liquid-state lithium-oxygen micro-battery by scanning transmission electron microscopy,” Scientific Reports (2018) Abstract
Jeung Hun Park, Nicholas M. Schneider, Daniel A. Steingart, Hariklia Deligianni, Suneel Kodambaka, and Frances M. Ross. “Control of Growth Front Evolution by Bi Additives during ZnAu Electrodeposition,” Nano Letters (2018) Abstract
YuBo Wang, Shuai Wang, and Xing Lu. “In Situ Observation of the Growth of ZnO Nanostructures Using Liquid Cell Electron Microscopy,” The Journal of Physical Chemistry C (2017) Abstract
Mingyuan Ge, Ming Lu, Yong Chu & Huolin Xin. “Anomalous Growth Rate of Ag Nanocrystals Revealed by in situ STEM,” Scientific Reports (2017) Abstract
See Wee Chee, Shu Fen Tan, Zhaslan Baraissov, Michel Bosman & Utkur Mirsaidov. “Direct observation of the nanoscale Kirkendall effect during galvanic replacement reactions,” Nature Communications (2017) Abstract
Eli Fahrenkrug, Daan Hein Alsem, Norman Salmon and Stephen Maldonado. “Electrochemical Measurements in In Situ TEM Experiments,” Journal of The Electrochemical Society (2017) Abstract
 Fei-Hu Du, Yizhou Ni, Ye Wang, Dong Wang, Qi Ge, Shuo Chen, and Hui Ying Yang. “Green Fabrication of Silkworm Cocoon-like Silicon-Based Composite for High-Performance Li-Ion Batteries,” ACS Nano (2017) Abstract
 Chuchu Yang, Jiuhui Han, Pan Liu, Chen Hou, Gang Huang, Takeshi Fujita, Akihiko Hirata, and Mingwei Chen. “Direct Observations of the Formation and Redox-Mediator-Assisted Decomposition of Li2O2 in a Liquid-Cell Li–O2 Microbattery by Scanning Transmission Electron Microscopy,” Advanced Materials (2017) Abstract
 Karalee Jarvis, Chih-Chieh Wang, María Varela, Raymond R. Unocic, Arumugam Manthiram, and Paulo J. Ferreira. “Surface Reconstruction in Li-rich Layered Oxides of Li-ion Batteries,” Chemsitry of Materials (2017) Abstract
 Edward R. White, Jared J. Lodico & B. C. Regan. “Intercalation events visualized in single microcrystals of graphite,” Nature Communications (2017)   Abstract
 Jeung Hun Park, Daniel A. Steingart, Suneel Kodambaka, and Frances M. Ross. “Electrochemical electron beam lithography: Write, read, and erase metallic nanocrystals on demand,” Science Advances (2017)   Abstract
 Timothy S. Arthur, Per-Anders Glans, Nikhilendra Singh, Oscar Tutusaus, Kaiqi Nie, Yi-Sheng Liu, Fuminori Mizuno, Jinghua Guo, Daan Hein Alsem, Norman J. Salmon, and Rana Mohtadi. “Interfacial insight from operando sXAS/TEM for magnesium metal deposition with borohydride electrolytes,” Chemistry of Materials (2017)   Abstract
 J. Lim,Y. Li, D. H. Alsem, H. So, S. C. Lee, P. Bai, D.A. Cogswell, X. Liu, N. Jin, Y. Yu, N. J. Salmon, D. A. Shapiro, M. Z. Bazant, T.Tyliszczak, W. C. Chueh, “Origin and Hysteresis of Lithium Compositional Spatiodynamics Within Battery Primary Particles,” Science (2016)   Abstract
 Yimin A. Wu, Liang Li, Zheng Li, Alper Kinaci, Maria K. Y. Chan, Yugang Sun, Jeffrey R. Guest, Ian McNulty, Tijana Rajh, and Yuzi Liu. “Visualizing Redox Dynamics of a Single Ag/AgCl Heterogeneous Nanocatalyst at Atomic Resolution,” ACS Nano (2016)  Abstract
 J.H. Park, N.M. Schneider, J.M. Grogan, M.C. Reuter, H.H. Bau, S. Kodambaka & F.M. Ross, “Control of Electron Beam-Induced Au Nanocrystal Growth Kinetics
through Solution Chemistry,” Nano Letters (2015)
Abstract
Raymond R. Unocic, Loïc Baggetto, Gabriel M. Veith, Jeffery A. Aguiar, Kinga A. Unocic, Robert L. Sacci, Nancy J. Dudney and Karren L. More. “Probing battery chemistry with liquid cell electron energy loss spectroscopy,” Chemical Communications (2015) Abstract
 M. Ge, Y. Lu, P. Ercius, J. Rong, X. Fang, M. Mecklenburg, and C. Zhou “Large-Scale Fabrication, 3D Tomography, and Lithium-Ion Battery Application of Porous Silicon” Nano Letters (2014) Abstract
 R.L. Sacci, N. Dudney, K. More, L.R. Parent, I. Arslan, N.D. Browning, and R.R. Unocic. “Direct Visualization of Initial SEI Morphology and Growth Kinetics During Lithium Deposition by In-Situ Electrochemical Transmission Electron Microscopy,” Chemical Communication (2014) Abstract
 P. Abellan, B. L. Mehdi, L.R. Parent, M. Gu, C. Park, W. Xu, Y. Zhang, I. Arslan, J.G. Zhang, C.M. Wang, J.E. Evans, and N.D. Browning. “Probing the Degradation Mechanisms in Electrolyte Solutions for Li-Ion Batteries by in Situ Transmission Electron Microscopy,” Nano Letters (2014) Abstract
 M. Gu, L.R. Parent, B.L. Mehdi, R.R. Unocic, M.T. McDowell, R.L. Sacci, W. Xu, J.G. Connell, P. Xu, P. Abellan, X. Chen,Y. Zhang, D.E. Perea, J.E. Evans, L.J. Lauhon, J.G. Zhang, J. Liu, N.D. Browning, Y. Cui, I. Arslan, and C.M. Wang. “Demonstration of an Electrochemical Liquid Cell for Operando Transmission Electron Microscopy Observation of the Lithiation/Delithiation Behavior of Si Nanowire Battery Anodes.” Nano Letters (2013) Abstract
E.R. White, S.B. Singer, V. Augustyn, W.A. Hubbard, M. Mecklenburg, B. Dunn, and B.C. Regan,“In-Situ Transmission Electron Microscopy of Lead Dendrites and Lead Ions in Aqueous Solution,” ACS Nano (2012) Abstract
C.M. Wang, W. Xu, J. Liu, D.W. Choi, B. Arey, L.V. Saraf, J.G. Zhang, Z.G. Yang, S. Thevuthasan, D.R. Baer and N. Salmon. “In situ transmission electron microscopy and spectroscopy studies of interfaces in Li ion batteries: Challenges and opportunities,” Journal of Materials Research (2010) Abstract

 

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